US11195634B2 - Angstrom-scale nanowire arrays in zeolite - Google Patents
Angstrom-scale nanowire arrays in zeolite Download PDFInfo
- Publication number
- US11195634B2 US11195634B2 US16/287,721 US201916287721A US11195634B2 US 11195634 B2 US11195634 B2 US 11195634B2 US 201916287721 A US201916287721 A US 201916287721A US 11195634 B2 US11195634 B2 US 11195634B2
- Authority
- US
- United States
- Prior art keywords
- zeolite
- mixture
- angstrom
- nanowire arrays
- nanowires
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active, expires
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/54—Phosphates, e.g. APO or SAPO compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/05—Light metals
- B22F2301/052—Aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/30—Low melting point metals, i.e. Zn, Pb, Sn, Cd, In, Ga
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2304/00—Physical aspects of the powder
- B22F2304/05—Submicron size particles
- B22F2304/052—Particle size below 1nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- Metal nanowires such as aluminum nanowires
- metal nanowires have received great attention due to their potential applications in manufacturing capacitors, electrochemical biosensors, photovoltaic systems, interconnects, and hydrogen storage.
- metal nanowires are incorporated to semiconducting nanowires, new functions for metal-semiconductor devices and superconductor-semiconductor devices can be developed.
- porous anodic aluminum oxide was attached to the conductive substrate as templates to synthesize aluminum nanowires for fabricating vertically-oriented aluminum nanowire arrays.
- AAO anodic aluminum oxide
- CVD chemical vapor preposition
- lithographical method and stress-induced spontaneous growth were also used for fabricating aluminum nanowires. Nevertheless, the average diameters of aluminum nanowires were in the range of several tens to a few hundred nanometers. Moreover, the separation between adjacent aluminum nanowires was of a scale of microns, leading to a rather low density of the aluminum nanowires arrays. As a result, the quantum properties, such as superconductivity, of the aluminum nanowires fabricated were similar to these of the bulk aluminum.
- Embodiments of the subject invention pertain to a composite material of Angstrom-scale nanowire arrays prepared by using zeolite as a template.
- a method for fabricating Angstrom-scale aluminum nanowire arrays can comprise mixing aluminum and zeolite crystals with a predetermined weight ratio; heating the mixture under a first predetermined condition(s); cooling down the mixture; heating the mixture under a second predetermined condition(s); and cooling down the mixture to obtain Angstrom-scale aluminum nanowire arrays.
- the predetermined weight ratio of zeolite crystals and aluminum can be about 1:9.
- the heating the mixture under a first predetermined condition(s) can comprise heating the mixture at about 800° C. under a pressure of about 400 Torr for about 6 hours in an oxygen atmosphere.
- the heating the mixture under a second predetermined condition(s) can comprise heating the mixture at a temperature in a range between about 660° C. and about 900° C. under a pressure in a range between 100 Torr and about 1600 Torr for about 3 hours in an inert gas atmosphere.
- the Angstrom-scale aluminum nanowire arrays obtained can have an average diameter smaller than 1 nm.
- a method for preparing Angstrom-scale metal nanowire arrays by using zeolite crystals as templates can comprise mixing liquid metal and zeolite crystals; heating the mixture under a first predetermined condition(s); and cooling down the mixture to obtain Angstrom-scale metal nanowire arrays.
- the liquid metal is gallium (Ga)
- the mixture can be heated at a temperature of about 80° C. under a pressure smaller than 100 bar.
- the liquid metal is zinc (Zn)
- the mixture can be heated at a temperature of about 500° C. under a pressure smaller than 100 bar.
- the cooling down the mixture can comprise cooling down the mixture by liquid nitrogen.
- a method for preparing Angstrom-scale carbon nanowire arrays using zeolite crystals as templates can comprise mixing methane (CH 4 ) and zeolite crystals; heating the mixture under a first predetermined condition(s); and cooling down the mixture to obtain the Angstrom-scale carbon nanowire arrays.
- the heating the mixture under a first predetermined condition(s) can comprise heating the mixture at a temperature of about 1000° C. under a pressure of about 6 atmospheres for about 10 hours.
- a composite material of Angstrom-scale nanowires in zeolite can comprise zeolite having porous structures; and a plurality of nanowires having an average diameter smaller than 1 nm and dispersed on internal or external surfaces of the porous structures.
- the plurality of nanowires is made of any one of aluminum (Al), gallium (Ga), zinc (Zn), and carbon (C).
- the porous structures can have an average pore size of about 0.74 nm.
- FIG. 1 is a flow diagram illustrating a process for synthesizing zeolite, according to an embodiment of the subject invention.
- FIG. 2 is schematic illustration of a process for fabricating aluminum nanowires by using the zeolite synthesized as shown in FIG. 1 as a template, according to an embodiment of the subject invention.
- FIG. 3 is a schematic illustration of a process of liquid aluminum penetrating into linear pores of a zeolite template according to an embodiment of the subject invention.
- FIG. 4 shows Scanning Electron Microscope (SEM) images of aluminum nanowires in micro-platelet shaped zeolite template crystals according to an embodiment of the subject invention.
- FIG. 5 shows X-ray Diffraction (XRD) spectra of aluminum nanowires in micro-platelet shaped zeolite template crystals with a wavelength of 1.540562 ⁇ for Cu-K ⁇ radiation according to an embodiment of the subject invention.
- XRD X-ray Diffraction
- FIG. 6 shows Raman spectra of aluminum nanowires in micro-platelet shaped zeolite template crystals with excitation laser wavelength of 514.5 nm measured at room temperature, according to an embodiment of the subject invention.
- FIG. 7 is a schematic illustration of four-terminal geometry etched by the FIB of a platelet crystal of aluminum nanowires in a zeolite template standing on its side, wherein two electrodes outside are current leads while two electrodes inside are potential leads, according to an embodiment of the subject invention.
- FIG. 8 shows an image of a four-terminal electrical measurement configuration taken by the FIB, wherein a constant current is supplied with the voltage probes measuring the voltage drop across a very narrow gap (for example, about 100 nm), according to an embodiment of the subject invention.
- FIG. 9 illustrates resistance as a function of temperature for a first sample of the aluminum nanowires in micro-platelet shaped zeolite template crystals, measured in the four-terminal configuration, according to an embodiment of the subject invention.
- FIG. 10 illustrates differential resistance of a first sample of aluminum nanowires in micro-platelet shaped zeolite template crystals as a function of bias current at different temperatures according to an embodiment of the subject invention.
- FIG. 11 a is a schematic illustration of the four-terminal geometry on ab plane perpendicular to an axial direction of aluminum nanowires in micro-platelet shaped zeolite template crystals, according to an embodiment of the subject invention.
- FIG. 11 b is an image of the four-terminal electrical measurement configuration on ab plane taken by the FIB according to an embodiment of the subject invention.
- FIG. 12 illustrates temperature dependency of resistance for a second sample of the aluminum nanowires in micro-platelet shaped zeolite template crystals measured by the four-terminal configuration on ab plane, according to an embodiment of the subject invention.
- FIG. 13 illustrates magnetoresistance of the second sample of the aluminum nanowires in micro-platelet shaped zeolite template crystals measured by the four-terminal configuration on ab plane, wherein an applied magnetic field is in parallel to an axial direction of the aluminum nanowires in zeolite, according to an embodiment of the subject invention.
- FIG. 14 illustrates differential resistance of the second sample of the aluminum nanowires in micro-platelet shaped zeolite template crystals as a function of bias current at different temperatures, according to an embodiment of the subject invention.
- FIG. 15 a illustrates DC magnetization of Ga nanowires in zeolite, wherein magnetic moment is shown as a function of temperature for an external magnetic field of 20 Oe under ZFC and FC conditions, according to an embodiment of the subject invention.
- FIG. 15 b illustrates DC magnetization of Ga nanowires in zeolite, wherein magnetization hysteresis loops are shown at different temperatures according to an embodiment of the subject invention.
- FIG. 16 a illustrates DC magnetization of Zn nanowires in zeolite showing the ZFC and FC magnetic moment according to an embodiment of the subject invention.
- FIG. 16 b illustrates DC magnetization of Zn nanowires in zeolite, wherein magnetization hysteresis loops are shown at different temperatures according to an embodiment of the subject invention.
- FIG. 17 a illustrates the specific-heat data for Ga nanowires in zeolite and Zn nanowires in zeolite, showing the electronic specific heat of nanowires in zeolite together with a fit to the alpha model, wherein the insert shows the total specific heat in 0 and 0.3 T, which represents the superconducting and normal state, respectively, according to an embodiment of the subject invention.
- FIG. 17 b illustrates the specific-heat data for Ga nanowires in zeolite and Zn nanowires in zeolite, showing the electronic specific heat of Zn nanowires in zeolite together with a fit to the alpha model, wherein the insert shows the total specific-heat in different applied magnetic fields, according to an embodiment of the subject invention.
- FIG. 18 a illustrates superconducting phase diagrams of Ga nanowires in zeolite, wherein a fit with the standard Werthamer, Helfand and Hohenberg (WHH) model for the upper critical field of a type-II superconductor is added, according to an embodiment of the subject invention.
- WH Hohenberg
- FIG. 18 b illustrates superconducting phase diagrams of Zn nanowires in zeolite, wherein a fit with the standard Ginzburg-Landau model for the critical field of a type-I superconductor, according to an embodiment of the subject invention.
- FIG. 19 shows Raman spectra of carbon nanowires in zeolite, according to an embodiment of the subject invention.
- FIG. 20 shows weight percentage as a function of temperatures of thermogravimetric analysis (TGA) of carbon nanowires in zeolite according to an embodiment of the subject invention.
- TGA thermogravimetric analysis
- FIG. 21 shows electrical conducting properties of carbon nanowires in zeolite according to an embodiment of the subject invention.
- Embodiments of the subject invention pertain to a composite material of Angstrom-scale well-ordered nanowire arrays in zeolite and its fabrication methods.
- the Angstrom-scale nanowire arrays can be prepared by using zeolite as a template.
- the zeolite template can be prepared by a hydrothermal method to obtain porous structures with an average pore size of 0.74 nm to ensure the diameters of nanowire arrays thereafter prepared to be of an Angstrom scale.
- the Angstrom-scale nanowire arrays can be made of a variety of materials including, hut are not limited to, aluminum (Al), gallium (Ga), zinc (Zn), carbon (C), indium (In), or magnesium (Mg).
- Al aluminum
- Ga gallium
- Zn zinc
- C carbon
- In indium
- Mg magnesium
- the composite material of the nanowire arrays in zeolite can exhibit superior characteristics of one-dimensional (1D) superconductors.
- a zeolite template such as SAPO-5 zeolite with an AFI topology, or other zeolites with one-dimensional channels, can be used as a template to fabricate the metal nanowires such as aluminum nanowires, gallium nanowires, indium nanowires, magnesium nanowires, or zinc nanowires, as well as carbon nanowires.
- zeolite templates having a framework other than AFI topology such as FAU, LTL, ABW, can also be used to fabricate nanowires of Angstrom scale or nanometer scale.
- a zeolite template for example, SAPO-5 zeolite with an AFI topology
- a hydrothermal method for example, SAPO-5 zeolite with an AFI topology
- the synthesis ingredients include aluminum oxide (Al 2 O 3 ), phosphorus pentoxide (P 2 O 5 ), silicon dioxide (S i O 2 ), triethanolamine (TEA), and deionized (DI) water.
- a molar ratio of Al 2 O 3 :P 2 O 5 :S i O 2 :TEA:H 2 O can be 1:0.8:1:3.5:50.
- the zeolite can be synthesized by the following steps:
- FIG. 1 shows an exemplary process for synthesizing the zeolite crystals, according to an embodiment of the subject invention.
- step S 100 about 5.68 g of phosphoric acid (H 3 PO 4 ) (for example, H 3 PO 4 of 85% from Panreac) is mixed with about 22.8 ml of deionized (DI) water to form a solution.
- step S 105 the solution is placed in an ice-water bath and about 4.42 g of pseudoboehmite (for example, Catapal A from SASOL) is added to the solution to obtain a mixture, and the mixture is stirred for about one hour.
- pseudoboehmite for example, Catapal A from SASOL
- step S 110 about 4.62 g of a silica solution (for example, Ludox HS-40 having 40 wt % from Sigma-Aldrich) is added to the mixture of the step of S 105 and the mixture is stirred for about another 1 hour. Further, at step S 115 , the resulting solution of the step S 110 is taken out of the ice-water bath and stirred for about 12 hours at room temperature to form a uniform precursor gel.
- a silica solution for example, Ludox HS-40 having 40 wt % from Sigma-Aldrich
- the precursor gel obtained from the step S 115 is transferred to a container, for example a Teflon autoclave having a capacity of 100 ml, and the container is placed in an oven (for example, MARS-5 from CEM with maximum power of 1600 W).
- the precursor gel is rapidly heated to about 180° C. within about 1.5 minutes with a heating power of, for example, 1600 W.
- the precursor gel is maintained in the container at that temperature of about 180° C. for a duration of about 2.5 hours with a heating power of, for example, 400 W.
- step S 130 the precursor gel is cooled to room temperature to obtain the zeolite.
- the zeolite is washed at step S 135 , is collected by a means of separation, for example, centrifugation at step S 140 ; and is dried at about 120° C. at step S 145 .
- the resulting zeolite can have micro-platelet shaped crystals having a hexagonal shape, with a thickness of about 2 microns and a lateral dimension in a range of 6-10 microns.
- zeolites are aluminosilicate or aluminophosphate compounds having very regular molecular structures containing pores.
- the framework of the zeolite synthesized as described above can comprise alternating tetrahedral (AlO_4) ⁇ circumflex over ( ) ⁇ and (PO_4) ⁇ circumflex over ( ) ⁇ + that form linear channels.
- AlO_4 alternating tetrahedral
- PO_4 ⁇ circumflex over ( ) ⁇ +
- ab plane the plane perpendicular to c-axis
- the linear channels of the zeolite can exhibit a triangular lattice structure in the ab plane with a center-to-center separation of about 1.37 nm between the nearest channels.
- the crystals of the zeolite synthesized can be electrically insulating and optically transparent from ultraviolet to the near infrared, and thermally stable up to 1200° C.
- the c-axis of the crystals can be perpendicular to the platelet surface.
- the crystals of the zeolite template synthesized as described above are heated at about 800° C. under a pressure of about 400 Torr in oxygen atmosphere for a duration of about 6 hours to remove the TEA precursors inside the zeolite template crystals.
- the aluminum powder and the zeolite template crystals are uniformly mixed and pressed into a disk by using a box having four lateral sides fixed but with top side or bottom side movable, so as to facilitate applying pressure to the mixture.
- the resulting mixture is placed in a heating apparatus such as an oven and heated in a temperature range between about 660° C. and about 900° C., preferably at a temperature between about 750° C. and about 850° C., under a pressure in a range between about 100 Torr and about 1600 Torr, preferably at a pressure of about 800 Torr, in an inert gas (for example, argon or nitrogen) atmosphere for about 3 hours.
- the inert gas is used as protecting gas because aluminum can be easily oxidized.
- the melting point of aluminum is at about 660° C.
- the aluminum powder melts and penetrates into linear channels of the zeolite template.
- the melted liquid aluminum has to overcome the surface tension of the liquid aluminum.
- the surface tension of the liquid aluminum linearly decreases with increasing temperatures. Therefore, in one embodiment, the temperature of the oven is adjusted and a pressure in a range of 1 kPa to 100 kPa is applied to the oven to improve the pore filling factor of the resulting aluminum nanowire arrays in the zeolite.
- the liquid aluminum is solidified inside the linear channels of the zeolite template to form the composite material of aluminum nanowire arrays in zeolites.
- the preferred optimal condition of the aluminum penetrating process is 850° C. with a pressure of 800 Torr.
- diameters of the aluminum nanowires obtained by using the zeolite template are close to the pore size (for example, 0.74 nm) of the zeolite template crystals.
- FIG. 3 shows a process of the liquid aluminum penetrating into the linear pores of the zeolite template crystals and forming stable structure due to the attractive force between aluminum atoms and oxygen atoms on the channel walls of the zeolite template crystals, according to an embodiment of the subject invention.
- the zeolite template crystals synthesized have porous structures with an average pore size of about 0.74 nm.
- the plurality of nanowire arrays dispersed on internal or external surfaces of the porous structures can have an average diameter smaller than 1 nm.
- the composite material of the aluminum nanowire arrays in zeolite fabricated as described above are characterized by different methods, such as scanning electron microscope (SEM), X-ray diffraction (XRD), Raman spectra, energy-dispersive spectroscopy (EDX) and conductivity measurement.
- SEM scanning electron microscope
- XRD X-ray diffraction
- EDX energy-dispersive spectroscopy
- FIG. 4 shows Scanning Electron Microscope (SEM) images of aluminum nanowires embedded in micro-platelet shaped zeolite template crystals according to an embodiment of the subject invention.
- the structure of the Angstrom-scale aluminum nanowires in zeolite is characterized by X-ray diffraction (XRD) with Cu-K ⁇ radiation (for example, by Philips PW1830).
- the XRD pattern is recorded in a 2 ⁇ ranging of 10°-90 with a scan step of 0.03° at grazing incidence angle (for example 3°).
- the wavelength of Cu-K ⁇ radiation can be 1.540562 ⁇ .
- the first small peak is around 21° and the second small peak is around 22°, both resulting from the zeolite template.
- the other peaks that originated from the Angstrom-scale aluminum nanowires are labeled as (111), (200), (220), and (311) in FIG. 5 .
- the Miller index of the third peak at 38.48° is labeled as (111)
- the fourth peak at 44.91° is labeled as (200)
- the fifth peak at 65.22° is labeled as (220)
- the sixth peak at 78.30° is labeled as (311). It is noted that the intensity of the peak (111) is the strongest in FIG. 5 .
- FIG. 6 illustrates Raman spectroscopy of the Angstrom-scale aluminum nanowires in zeolite performed at room temperature by Micro-Raman (for example, a Renishaw InVia Confocal Raman microscope) with laser wavelength of 514.5 nm.
- Micro-Raman for example, a Renishaw InVia Confocal Raman microscope
- laser wavelength 514.5 nm.
- the aluminum nanowire arrays in zeolite can have a core-shell structure, where the core is the aluminum nanowire and the shell is the layer of aluminum oxide.
- the conducting property of the Angstrom-scale aluminum nanowire arrays in zeolite is measured.
- the sample preparation process for the measurement is described below.
- a thin layer of photoresist for example, 950 PMMA 9 A
- crystals of the aluminum nanowire arrays in zeolite are dispersed on the photoresist and heated on a heating apparatus such as a hotplate at about 180° C. for about 90 seconds.
- a heating apparatus such as a hotplate at about 180° C. for about 90 seconds.
- the crystals are fixed on the surface of the glass film substrate in order to facilitate the subsequent process.
- a crystal standing on its side is selected.
- a layer of titanium of a thickness (for example, 5 nm) is sputtered on the side surface of the micro-platelet sample crystal selected and another layer of gold of a thickness (for example, 60 nm) is sputtered above the titanium layer.
- a focused ion beam is used to select one crystal of the aluminum nanowire arrays in zeolite. It is noted that the surface layer of the aluminum nanowire arrays in zeolite is etched by the FIB, since it is already oxidized by oxygen. Next, a layer of platinum (Pt) is sputtered on the etched area by the FIB as an electrode. Then, the FIB is used to make a four-terminal configuration as shown in FIG. 7 . The interval between different electrodes is about 100 nm.
- FIG. 8 is an image of the four-terminal electrical measurement configuration taken by the FIB.
- a constant current is supplied by voltage probes measuring the voltage drop across a very narrow gap (for example, about 100 nm), according to an embodiment of the subject invention.
- FIG. 9 illustrates temperature dependency of resistance for a first sample S 1 of the Angstrom-scale aluminum nanowire arrays in zeolite measured in the four-terminal configuration with a current of 500 nA.
- the resistance is linearly decreased from about 3.6 ⁇ to about 2.7 ⁇ , when the temperature is decreased from room temperature (about 300 K) to about 100 K. It is noted that the resistance is decreased at a faster rate when the temperature is decreased from about 100 K to about 50 K.
- the resistance starts to drop smoothly but does not reach a resistance of zero when temperature is decreased to about 2 K, indicating a one-dimensional (1D) superconducting transition is achieved.
- Another feature of superconductivity is nonlinear current-voltage characteristic observed below one-dimensional superconducting transition temperature.
- FIG. 10 illustrates current dependency of differential resistance at different temperatures.
- the differential resistance is increased from 1.7 ⁇ to 2.5 ⁇ when the bias current is increased from 0 ⁇ A to 100 ⁇ A, indicating that the superconductivity of the Angstrom-scale aluminum nanowire arrays is suppressed by a large bias current.
- the drop in the differential resistance curve becomes more and more moderate when the temperature is increased from about 2 K to about 100 K; and the drop in the differential resistance curve is negligible after the temperature goes higher than 50 K.
- FIG. 11 a illustrates the four-terminal geometry on ab plane perpendicular to an axial direction of the aluminum nanowires in micro-platelet shaped zeolite template crystals, according to an embodiment of the subject invention.
- FIG. 11 b illustrates the four-terminal electrical measurement configuration on ab plane taken by the FIB according to an embodiment of the subject invention.
- the temperature dependency of the resistance for a second sample S 2 of the Angstrom-scale aluminum nanowire arrays in zeolite measured by the four-terminal geometry with a constant current of 500 nA is shown. It is noted that the resistance is increased slightly from about 8.8 ⁇ to about 9.0 ⁇ , when the temperature is decreased from about 300 K to about 50 K. Then, the resistance starts to decrease sharply but smoothly, when the temperature is decreased from about 50 K to about 2 K.
- the magnetoresistance of the Angstrom-scale aluminum nanowire arrays is also measured by the four-terminal configuration on ab plane.
- the resistance of the second sample S 2 is increased smoothly but only slightly, as shown in FIG. 13 .
- FIG. 14 illustrates the dependency between current and differential resistance for the second sample S 2 .
- a temperature of about 10 K there is a well-defined resistance drop at a bias current of zero, indicating superconductivity. This drop becomes more and more moderate when the temperature is increased from about 2 K to about 80 K and the drop in the differential resistance curve is negligible after the temperature goes higher than 50 K, indicating that the transition temperature of superconducting is around 50 K.
- These measurement results of differential resistance of the second sample S 2 are consistent with the measurement results of the first sample S 1 .
- the Angstrom-scale aluminum nanowire arrays fabricated by using zeolite template can have a very high density, since the separation between adjacent aluminum nanowires can be as little as 1.4 nm.
- micro-platelet zeolites with linear channels synthesized by the hydrothermal method as described above can be used as templates for fabrication of Angstrom-scale Gallium (Ga) nanowires and Angstrom-scale Zinc (Zn) nanowires.
- the ingredients used in the zeolite template synthesis can include, but not limited to, aluminum oxide, phosphorus pentoxide, silicon dioxide, triethanolamine (TEA), and deionized (DI) water.
- liquid Ga can be mixed with the zeolite template synthesized and then heated in a sealed container at a temperature of about 80° C. under a pressure up to about 100 bar. Then, the mixture is rapidly cooled by liquid nitrogen, resulting in Angstrom-scale Gallium (Ga) nanowires in zeolite.
- liquid Zn can be mixed with the zeolite template synthesized and then heated in a sealed container at a temperature of about 500° C. under a pressure up to about 100 bar. Then, the mixture is rapidly cooled by liquid nitrogen to obtain the Zinc (Zn) nanowires in zeolite.
- the gallium (Ga) or zinc (Zn) nanowires fabricated can infiltrate into the one-dimensional (1D) linear channels of the zeolite template such as AlPO-5 (AFI) having an internal pore diameter of about 7 ⁇ , and the gallium (Ga) or zinc (Zn) nanowires can be separated by an insulating wall of about 7-9 ⁇ .
- the zeolite template such as AlPO-5 (AFI) having an internal pore diameter of about 7 ⁇
- AFI AlPO-5
- the resulting Angstrom-scale Ga or Zn nanowire arrays in zeolite arranged in Josephson-coupled triangular arrays with an ab-plane lattice constant of 14.4 ⁇ , display superconductivity with Tc values of about 7.2 K and about 3.7 K, for Ga and Zn, respectively.
- the superconductivity with Tc values for the Angstrom-scale Ga or Zn nanowire arrays in zeolite are significantly enhanced by a factor of about 7 and about 4, in comparison to the superconductivity with Tc of bulk Ga or bulk Zn, respectively.
- the zeolite template of the composite superconductor dictates the nanostructure of Ga and Zn to be one-dimensional (1D) in the electronic sense, a highly advantageous effect for the superconducting pairing is achieved.
- the arrangement in a densely packed array structure of the Angstrom-scale Ga or Zn nanowire in zeolite inhibits coherence being completely suppressed by strong phase fluctuations as in other conventional one-dimensional (1D) superconductors.
- Cooper pairs are confined in Ga or Zn nanowire arrays with thicknesses of only a few hundred picometers.
- the nanowire arrays of an Angstrom-scale almost approach the limit of a monoatomic chain and are in extremely close distance to each other.
- the nanowire arrays of Angstrom-scale form a regular array of almost crystalline quality.
- the bulk Ga or the bulk Zn is an elemental Bardeen-Cooper-Schrieffer (BCS) superconductor.
- BCS Bardeen-Cooper-Schrieffer
- the superconducting properties of the Angstrom-scale Ga or Zn nanowire arrays in zeolite are characterized by DC magnetization and by specific heat measurements as discussed below.
- FIG. 15 a shows the results of zero-field-cooled (ZFC) and field-cooled (FC) DC magnetizations of the Angstrom-scale Ga nanowire arrays in zeolite measured with a VSM SQUID magnetometer.
- the demagnetization factor of the sample is measured to be about 0.55.
- a clear Meissner effect is observed with onset at 7.7 K in a magnetic field of 20 Oe.
- Ga nanowires with one-dimensional nature of freestanding, are expected to have a rather gradual transition due to the phase slips. Therefore, the sharp transition of Ga nanowires observed in FIG. 15 a is attributed to the Josephson coupling between the nanowires.
- the ZFC data reveals the flux expulsion and subsequent flux treading as the temperature rises.
- the FC data show only partial flux expulsion.
- the ZFC and FC data also indicate that macroscopic screening currents can be formed in Ga nanowire arrays embedded in the insulating zeolite crystals, requiring transverse tunneling current between the Ga nanowires due to the Josephson coupling.
- the initial branch of the hysteresis loops first displays an almost linear behavior of the Meissner state before it passes through a minimum and then very slowly approaches the upper critical field (H_c2) at about 700 Oe at 1.8K.
- the critical field of the Ga nanowire arrays in zeolite is thus more than 100 times greater than that of the bulk Ga thanks to the effect of nanostructure, transforming the Ga nanowire arrays from a type-I superconductor to a type-II superconductor.
- FIGS. 16 a and 16 b the DC magnetization data of Zn nanowire arrays in zeolite are shown.
- both the ZFC and FC curves show a sharp Meissner effect below 3.7 K. Due to the stronger Meissner signal for Zn nanowire arrays in zeolite, the measurement can be performed in an applied field of only 1 Oe, in contrast to the greater field of 20 Oe required for the corresponding measurement of Ga nanowire arrays in zeolite.
- FIG. 16 b illustrates the M versus H diagram for the Zn nanowires at different temperatures.
- the shapes of these hysteresis curves differ significantly from these of Ga nanowire arrays in zeolite and the transition at the critical field for Zn is much sharper than that of the Ga nanowires.
- the curves of the Ga nanowire arrays in zeolite clearly shows typical behaviors of a type-II superconductor, while the field dependent magnetization of Zn nanowire arrays in zeolite could on first view be interpreted as that of a superconductor at the borderline between a type-I superconductor and a type-II superconductor.
- the Zn nanowire arrays in zeolite is determined to be a type-I superconductor.
- a type-I superconductor with ideal demagnetization factor one would expect that the Meissner screening would have vanished abruptly at the critical field thus forming saw-tooth like shapes of curves in the M versus H diagram.
- the critical field transition of the Zn nanowire arrays in zeolite appears quite broad instead is attributed to the non-ideal demagnetization factor of about 0.6 of the sample of the Zn nanowire arrays in zeolite, which causes the intermediate state (not the Abrikosov state of type-II superconductors) with partial field penetration to occur, rendering the critical field transition into a broad step.
- the specific heat of the Ga nanowire arrays in zeolite and of the Zn nanowire arrays in zeolite are measured with a calorimeter, respectively.
- the first term is the electronic contribution of the Ga nanowire arrays in zeolite or of the Zn nanowire arrays in zeolite with the Sommerfeld constant ⁇ n , as denoted by C elect. below; and the second term is the low-temperature expansion of the lattice specific heat according to the Debye model.
- FIG. 17 a shows C elect /T of the Ga nanowire arrays in zeolite
- FIG. 17 b shows C elect /T of the Zn nanowire arrays in zeolite.
- the transition midpoint is at about 7 K, but with a fluctuation tail up to about 7.7 K.
- the midpoint occurs at about 3.86 K.
- the superconducting contribution to the specific heat of the Ga nanowires is extremely low. ⁇ C represents only 0.3% of the total specific heat.
- the Ga nanowires in zeolite therefore may not be suitable for applications due to the very low filling factor of the zeolite pores. Nevertheless, the superconducting transition is significantly sharp and the composite material can produce a significant Meissner effect.
- the superconducting transition anomaly ⁇ C of the Zn nanowire arrays in zeolite represents 23% of the total specific heat of the composite material and is therefore clearly visible in the graph of the total specific heat without the need to subtract background data.
- Such a large ratio between ⁇ C and the normal state background is only possible, if the Zn nanowire arrays in zeolite has an almost perfect pore filling factor and the nanowires form a homogeneous and highly dense arrays.
- the Josephson coupling between the nanowires is so strong that the Zn nanowire arrays in zeolite sample remains a type-I superconductor, as can be seen from the sharp peaks sitting on top of the specific heat jumps at Tc.
- This observation is typical for type-I superconductors, for which the superconducting transition becomes of a first-order nature in any finite magnetic field.
- the residual magnetic field in the superconducting magnet cryostat used is carefully compensated, the peak does not vanish when approaching zero field, which is most likely due to the Earth's magnetic field, which is almost perpendicular to the axis of the superconducting magnet which is located in Hong Kong, where the test was conducted and hence cannot be compensated.
- the superconducting phase diagrams for the Ga nanowire arrays in zeolite and the Zn nanowire arrays in zeolite are shown in FIGS. 18 a and 18 b , respectively.
- the diagrams are derived from the magnetization data.
- the diagrams are also derived from the specific heat.
- the temperature dependence of the upper critical field H c2 (T) is derived from the onset of the Meissner signal in the M(T) and M(H) data, while the midpoint of the jumps is used in the specific heat at T.
- the diagram of the Ga nanowire arrays in zeolite shows the characteristic magnetization hysteresis loops of a type-II superconductor.
- the model fits well with the data, except at high temperatures, where the data deviate towards higher temperatures. According to the results of the specific heat tests, this is attributed to the fluctuation tail above the superconducting main transition at 7 K.
- the lower critical field H c1 is normally obtained from the first deviation point from a linear behavior of the initial branch of the M(H) hysteresis loops.
- the Zn nanowire arrays in zeolite can be identified as a type-I superconductor based on the specific heat data.
- the temperature dependence of the critical field is determined as the upper onset of a Meissner effect in the M(H) data, and from the T c (H) value in the specific heat, which is determined from the centers of the specific heat jumps that occur just above the peaks.
- Angstrom-scale carbon nanowires can be fabricated by a chemical vapour deposition (CVD) method by using the zeolite templates synthesized by the hydrothermal method as described above.
- CVD chemical vapour deposition
- the zeolite templates are heated in 6 atmospheres of methane (CH 4 ), which is used as carbon source, at a temperature of about 1000° C. for about 10 hours.
- CH 4 methane
- the methane gas diffuses into the pores of the zeolite template and is decomposed due to the catalytic effect of the zeolite.
- the Angstrom-scale carbon nanowires are formed in the pores of the zeolite template.
- the optical and conducting properties of the Angstrom-scale carbon nanowires in zeolite are measured.
- the D band in the Raman spectra is obvious and the conductivity data show metallic behaviors of the Angstrom-scale carbon nanowires in zeolite in a temperature range from about 2 K to about 300 K. It is evident that the properties of the Angstrom-scale carbon nanowires in zeolite are quite different from these of the bulk carbon such as graphite.
- the Raman spectra are measured by a micro-Raman system (for example, JobinYvon T64000) with a laser wavelength of 514.5 nm.
- a micro-Raman system for example, JobinYvon T64000
- the zeolite template does not influence the Raman spectrum measurement of the Angstrom-scale carbon nanowires in zeolite, because the Raman signals of an empty zeolite template (control group) are much weaker than the Raman signals of the Angstrom-scale carbon nanowires in zeolite. Therefore, the Raman spectra of the Angstrom-scale carbon nanowires in zeolite can be measured.
- the peak around 1600 cm ⁇ 1 is the G band.
- the G band arises from the vibrations of carbon atoms in a hexagonal structure which are connected by C—C sp 2 bonds.
- the very high peak around 1350 cm ⁇ 1 is the D band which likely arises from the defects in the structure of the Angstrom-scale carbon nanowires in zeolite.
- the very high D band peak suggests that the structure of the Angstrom-scale carbon nanowires in zeolite is similar to that of graphene nanoribbon.
- the peak around 2700 cm ⁇ 1 is denoted as G′ band which originates from a second-order process.
- thermogravimetric analysis is used to assess the carbon content of the Angstrom-scale carbon nanowires in zeolite samples.
- samples of the Angstrom-scale carbon nanowires in zeolite are heated up in air from room temperature to about 800° C. with a heating rate of about 2° C./minute by a TGA device (for example, Q5000 TGA).
- the sample weight is constantly monitored by a microbalance. By burning off the carbon inside the zeolite crystals, the carbon contents from the difference in weight before and after the heating process are obtained.
- the carbon content of the Angstrom-scale carbon nanowires in zeolite is measured to be about 21.5 wt %.
- the derivative of the weight curve has a very sharp peak around 600° C., indicating that the decomposition temperature of the carbon nanowires structure inside the pores of the zeolite is around 600° C.
- the electrical conducting properties of the Angstrom-scale carbon nanowires are studied by fabricating devices from the CVD-heated samples of the Angstrom-scale carbon nanowires.
- the focused ion beam (FIB) is used to make the four-terminal configuration.
- Measurement of the fabricated device is carried out by a Physical Property Measurement System (PPMS).
- PPMS Physical Property Measurement System
- a Keithley 6221 is used as the current source and a SR850 lock-in is used as voltmeter to measure the resistance of the Angstrom-scale carbon nanowires.
- the resistivity of the Angstrom-scale carbon nanowires is measured to be 83.2 ⁇ m. Then, the resistivity of the Angstrom-scale carbon nanowires is compared with that of graphite. When the current is in parallel to a c-axis of the graphite, the resistivity is measured to be 2.5 ⁇ 5.0 ⁇ m. When the current is perpendicular to the c-axis, the resistivity is measured to be 3000 ⁇ m. Therefore, the resistivity of the Angstrom-scale carbon nanowires is between the resistivity of the parallel current and resistivity of the perpendicular current of the graphite.
- the resistivity of the Angstrom-scale carbon nanowires decreases linearly with temperature decrease, showing a metallic behavior. It is known that graphite is semiconducting at low temperatures and its resistivity increases with temperature decrease. Hence, the metallic behavior of the Angstrom-scale carbon nanowires at low temperatures is unexpected. Due to its superior conductivity, the Angstrom-scale carbon nanowires can be used as a material for electrodes of batteries.
- the subject invention includes, but is not limited to, the following exemplified embodiments.
- a method for fabricating Angstrom-scale aluminum nanowire arrays by using zeolite crystals as templates comprising steps of:
- heating the mixture under a first predetermined condition(s) comprises heating the mixture at a temperature of about 800° C. under a pressure of about 400 Torr for about 6 hours in an oxygen atmosphere.
- heating the mixture under a second predetermined condition(s) comprises heating the mixture at a temperature in a range between about 660° C. and about 900° C. under a pressure in a range between 100 Torr and about 1600 Torr for about 3 hours in an inert gas atmosphere.
- a method for preparing Angstrom-scale metal nanowire arrays by using zeolite crystals as templates comprising steps of:
- cooling down the mixture comprises cooling down the mixture by liquid nitrogen.
- a method for preparing Angstrom-scale carbon nanowire arrays by using zeolite crystals as templates comprising steps of:
- heating the mixture under a first predetermined condition(s) comprises heating the mixture at a temperature of about 1000° C. under a pressure of about 6 atmospheres for about 10 hours.
- a method for preparing zeolite comprising steps of:
- heating the precursor gel to form a solid product comprises:
- a composite material of Angstrom-scale nanowires in zeolite comprising:
- the composite material according to embodiment 18, wherein the plurality of nanowires is made of any one of aluminum (Al), gallium (Ga), zinc (Zn), and carbon (C).
- nanowire arrays have a core-shell structure having the aluminum nanowire as a core and the aluminum oxide layer as a shell.
- the composite material according to embodiment 25, wherein the Ga or Zn nanowire arrays in zeolite has superconductivity with T c values of about 7.2 K and about 3.7 K, for Ga and Zn, respectively.
- the composite material according to embodiment 25, wherein the Ga nanowire arrays in zeolite is a type-II superconductor.
- the composite material according to embodiment 19, wherein the plurality of nanowires is made of carbon and has metallic behaviors in term of resistivity.
- the composite material according to embodiment 19, wherein the plurality of nanowires is made of carbon and has metallic behaviors in term of resistivity.
Abstract
Description
-
- (1) mixing phosphoric acid (H3PO4) with deionized (DI) water;
- (2) mixing pseudoboehmite with the resulting solution in an ice-water bath with stirring adding silica solution to the mixture solution and stirring the mixture solution for a first predetermined period of time;
- (3) taking the mixture solution out of the ice-water bath and keeping stirring for a second predetermined period of time at a first predetermined temperature to form a uniform precursor gel;
- (4) heating the precursor gel to a second predetermined temperature at a first heating rate;
- (5) maintaining the precursor gel at the second predetermined temperature for a third predetermined period of time to form a solid product;
- (6) cooling the solid product to a third predetermined temperature to obtain the zeolite;
- (7) washing the resulting zeolite;
- (8) collecting the zeolite by a means of separation; and
- (9) drying the zeolite at a fourth predetermined temperature.
-
- mixing aluminum and zeolite crystals with a predetermined weight ratio;
- heating the mixture under a first predetermined condition(s);
- cooling down the mixture;
- heating the mixture under a second predetermined condition(s); and
- cooling down the mixture to obtain Angstrom-scale aluminum nanowire arrays.
-
- mixing liquid metal and zeolite crystals;
- heating the mixture under a first predetermined condition(s); and
- cooling down the mixture to obtain Angstrom-scale metal nanowire arrays.
-
- mixing methane (CH4) and zeolite crystals;
- heating the mixture under a first predetermined condition(s); and
- cooling down the mixture to obtain Angstrom-scale carbon nanowire arrays.
-
- mixing pseudoboehmite with a phosphoric acid (H3PO4) solution in an ice-water bath with stirring;
- adding a silica solution to the mixture solution;
- taking the resulting solution out of the ice-water bath;
- keeping stirring the resulting solution at room temperature for a predetermined time period to form a precursor gel;
- heating the precursor gel to form a solid product; and
- cooling the solid product to obtain the zeolite crystals.
-
- heating the precursor gel to a temperature at a temperature of about 180° C. within about 1.5 minutes; and
- maintaining at the temperature for about 2.5 hours.
-
- zeolite having porous structures; and
- a plurality of nanowires having an average diameter smaller than 1 nm and dispersed on internal or external surfaces of the porous structures.
- [1] P. Banerjee, I. Perez, L. Henn-Lecordier, S. B. Lee, and G. W. Rubloff,
Nature Nanotechnology 4, 292 (2009). - [2]J. Benson, S. Boukhalfa, A. Magasinski, A. Kvit, and G. Yushin,
ACS Nano 6, 118 (2012). - [3] B. Rizal, M. M. Archibald, T. Connolly, S. Shepard, M. J. Burns, T. C. Chiles, and M. J. Naughton,
Analytical Chemistry 85, 10040 (2013). - [4] R. Yu, K. L. Ching, Q. Lin, S. F. Leung, D. Arcrossito, and Z. Fan,
ACS Nano 5, 9291 (2011). - [5] T. H. Kim, X. G. Zhang, D. M. Nicholson, B. M. Evans, N. S. Kulkarni, B. Radhakrishnan, E. A. Kenik, and A. P. Li,
Nano Letters 10, 3096 (2010). - [6] W. Li, C. Li, H. Ma, and J. Chen, Journal of the American Chemical Society 129, 6710 (2007).
- [7] N. A. Melosh, A. Boukai, F. Diana, B. Gerardot, A. Badolato, P. M. Petroff, and J. R. Heath,
Science 300, 112 (2003). - [8] J. J. Wang, L. Chen, X. Liu, P. Sciortino, F. Liu, F. Walters, and X. Deng, Applied Physics Letters 89, 141105 (2006).
- [9] C. Ma, Y. Berta, and Z. Wang, Solid State Communications 129, 681 (2004).
- [10] J. W. Lee, M. G. Kang, B. S. Kim, B. H. Hong, D. Whang, and S. W. Hwang, Scripta Materialia 63, 1009 (2010).
- [11] S. T. Wilson, B. M. Lok, C. A. Messina, T. R. Cannan, and E. M. Flanigen, Journal of the American Chemical Society 104, 1146 (1982).
- [12] C. J. Jacobsen, C. Madsen, J. Houzvicka, I. Schmidt, and A. Carlsson, Journal of the American Chemical Society 122, 7116 (2000).
- [13] A. J. Yin, J. Li, W. Jian, A. J. Bennett, and J. M. Xu, Applied Physics Letters 79, 1039 (2001).
Claims (15)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US16/287,721 US11195634B2 (en) | 2018-02-28 | 2019-02-27 | Angstrom-scale nanowire arrays in zeolite |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201862636754P | 2018-02-28 | 2018-02-28 | |
US16/287,721 US11195634B2 (en) | 2018-02-28 | 2019-02-27 | Angstrom-scale nanowire arrays in zeolite |
Publications (2)
Publication Number | Publication Date |
---|---|
US20190267154A1 US20190267154A1 (en) | 2019-08-29 |
US11195634B2 true US11195634B2 (en) | 2021-12-07 |
Family
ID=67684028
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US16/287,721 Active 2039-12-25 US11195634B2 (en) | 2018-02-28 | 2019-02-27 | Angstrom-scale nanowire arrays in zeolite |
Country Status (1)
Country | Link |
---|---|
US (1) | US11195634B2 (en) |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050090387A1 (en) * | 2002-08-22 | 2005-04-28 | Koichi Niihara | Catalyst assembly |
US20060211802A1 (en) * | 2005-03-18 | 2006-09-21 | Soheil Asgari | Porous sintered metal-containing materials |
CN102951619A (en) | 2011-08-31 | 2013-03-06 | 深圳光启高等理工研究院 | Cadmium telluride nanowire and preparation method thereof |
CN103173832A (en) | 2013-04-25 | 2013-06-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Novel aluminum material with microscale self-driven dropwise condensation function and preparation method thereof |
CN103290465A (en) | 2013-05-15 | 2013-09-11 | 北京化工大学 | Method for preparing aluminum metal nanowires through high gravity technology |
US20160258069A1 (en) | 2015-03-03 | 2016-09-08 | The Trustees Of Boston College | Aluminum nanowire arrays and methods of preparation and use thereof |
US20170218518A1 (en) | 2003-01-31 | 2017-08-03 | Sigma Laboratories Of Arizona, Llc | Ultra-bright passivated aluminum nano-flake pigments |
US10683404B2 (en) * | 2015-11-17 | 2020-06-16 | Sabic Global Technologies B.V. | Porous polymer nanocomposites with ordered and tunable crystalline and amorphous phase domains |
-
2019
- 2019-02-27 US US16/287,721 patent/US11195634B2/en active Active
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050090387A1 (en) * | 2002-08-22 | 2005-04-28 | Koichi Niihara | Catalyst assembly |
US20170218518A1 (en) | 2003-01-31 | 2017-08-03 | Sigma Laboratories Of Arizona, Llc | Ultra-bright passivated aluminum nano-flake pigments |
US20060211802A1 (en) * | 2005-03-18 | 2006-09-21 | Soheil Asgari | Porous sintered metal-containing materials |
CN102951619A (en) | 2011-08-31 | 2013-03-06 | 深圳光启高等理工研究院 | Cadmium telluride nanowire and preparation method thereof |
CN103173832A (en) | 2013-04-25 | 2013-06-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Novel aluminum material with microscale self-driven dropwise condensation function and preparation method thereof |
CN103290465A (en) | 2013-05-15 | 2013-09-11 | 北京化工大学 | Method for preparing aluminum metal nanowires through high gravity technology |
US20160258069A1 (en) | 2015-03-03 | 2016-09-08 | The Trustees Of Boston College | Aluminum nanowire arrays and methods of preparation and use thereof |
US10683404B2 (en) * | 2015-11-17 | 2020-06-16 | Sabic Global Technologies B.V. | Porous polymer nanocomposites with ordered and tunable crystalline and amorphous phase domains |
Non-Patent Citations (26)
Title |
---|
Banerjee, P. et al., "Nanotublar metal-insulator-metal capacitor arrays for energy storage," Nature Nanotechnology, May 2009, 4:292-296. |
Benson, J. et al., "Chemical Vapor Deposition of Aluminum Nanowires on Metal Substrates for Electrical Energy Storage Applications," ACS NANO, 2012, 6(1): 118-125, American Chemical Society. |
Bogomolov et al. "Liquids in ultrathin channels (Filament and cluster crystals)", Sov. Phys. Usp. 21(1), Jan. 1978, pp. 77-83. * |
Cademartiri et al. "Ultrathin Nanowires—A Materials Chemistry Perspective", Adv. Mater. 2009, 21, 1013-1020. * |
Ding, X. et al., "In situ growth and characterization of Ag and Cu nanowires," Nanotechnology, 2006, 17:S376-S380, IOP Publishing Ltd. |
Gruev, V., "Fabrication of a dual-layer aluminum nanowires polarization filter array," Optics Express, Nov. 21, 2011, 19(24):1-9, Optical Society of America. |
Han, J. et al., "Confinement of Supported Metal Catalysts at High Loading in the Mesopore Network of Hierarchical Zeolites, with Access via the Microporous Windows," ACS Catalysis, 2018, 8:876-879, American Chemical Society. |
Inoue, S. et al., "Formation of Te Nanowires in Zeolite AFI and Their Polarized Absorption Spectra," International Journal of Modern Physics B, 2005, 19(15-17):2817-2822, World Scientific Publishing Company. |
Jacobsen, C. J. H. et al., "Mesoporous Zeolite Single Crystals," J. Am. Chem. Soc., 2000, 122:7116-7117, American Chemical Society. |
Kim, T. et al., "Large Discrete Resistance Jump at Grain Boundary in Copper Nanowire," Nano Letters, 2010, 10:3096-3100, American Chemical Society. |
Lee, J. W. et al., "Single crystalline aluminum nanowires with ideal resistivity," Scripta Materialia, 2010, 63:1009-1012, Elsevier Ltd. |
Li, W. et al.. "Magnesium Nanowires: Enhanced Kinetics for Hydrogen Absorption and Desorption," JACS Communications, 2007, 129:6710-6711, American Chemical Society. |
Ma, C. et al., "Patterned aluminum nanowires produced by electron beam at the surfaces of AIF3 single crystals," Solid State Communications, 2004, 129:681-685, Elsevier Ltd. |
Makita, T. et al., "Structures and electronic properties of aluminum nanowires," Journal of Chemical Physics, Jul. 1, 2003, 119(1):538-546, American Institute of Physics. |
Melosh, N. A. et al., "Ultrahigh-Density Nanowire Lattices and Circuits," Science, Apr. 4, 2003, 300:112-115. |
Rizal, B. et al., "Nanocoax-Based Electrochemical Sensor," Analytical Chemistry, 2013, 85:10040-10044, American Chemical Society. |
Romanov "Electronic structure of the minimum-diameter T, Pb and Bi quantum wire superlattices", J. Phys.: Condens. Matter 5, 1081-1090, 1993. * |
Shanenko, A. A. et al., "Size-dependent enhancement of superconductivity in Al and Sn nanowires: Shape-resonance effect," Physical Review B, 2006, 74:1-4, The American Physical Society. |
Singh, M. et al., "Synthesis and Superconductivity of Electrochemically Grown Single-Crystal Aluminum Nanowires," Chemistry of Materials, 2009, 21:5557-5559, American Chemical Society. |
Tolla, F. D. et al., "Electronic properties of ultra-thin aluminum nanowires," Surface Science, 2000, 454-456:947-951, Elsevier Science B.V. |
Wang, J. J. et al., "30-nm-wide aluminum nanowire grid for ultrahigh contrast and transmittance polarizers made by UV-nanoimprint lithography," Applied Physics Letters, 2006, 89:1-4, American Institute of Physics. |
Wilson, S. T. et al., "Aluminophosphate Molecular Sieves: A New Class of Microporous Crystalline Inorganic Solids," J. Am. Chem. Soc., 1982, 104:1146-1147, American Chemical Society. |
Yin, A. J. et al., "Fabrication of highly ordered metallic nanowire arrays by electrodeposition," Applied Physics Letters, Aug. 13, 2001, 79(7):1039-1041, American Institute of Physics. |
Yu, R. et al., "Strong Light Absorption of Self-Organized 3-D Nanospike Arrays for Photovoltaic Applications," ACS NANO, 2011, 5(11):9291-9298, American Chemical Society. |
Zgirski, M. et al., "Quantum fluctuations in ultranarrow superconducting aluminum nanowires," Physical Review B, 2008, 77:1-6, The American Physical Society. |
Zhang. B. et al., "Giant enhancement of superconductivity in arrays of ultrathin gallium and zinc sub-nanowires embedded in zeolite," Materials Today Physics, 2018, 6:38-44, Elsevier Ltd. |
Also Published As
Publication number | Publication date |
---|---|
US20190267154A1 (en) | 2019-08-29 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Luo et al. | In Situ transmission electron microscopy characterization and manipulation of two‐dimensional layered materials beyond graphene | |
Brun et al. | Review of 2D superconductivity: the ultimate case of epitaxial monolayers | |
Zhang et al. | Van der Waals epitaxial growth of 2D metallic vanadium diselenide single crystals and their extra‐high electrical conductivity | |
Xu et al. | Large-area high-quality 2D ultrathin Mo2C superconducting crystals | |
Zhou et al. | Large‐area and high‐quality 2D transition metal telluride | |
Xiao et al. | Simple synthesis of ultra-long Ag2Te nanowires through solvothermal co-reduction method | |
Hu et al. | Chemistry and physics in one dimension: synthesis and properties of nanowires and nanotubes | |
Palstra et al. | Superconductivity at 40K in cesium doped C60 | |
Wang et al. | Superconductivity in 4-Angstrom carbon nanotubes—A short review | |
Qi et al. | Thermoelectric devices based on one-dimensional nanostructures | |
Varlec et al. | Oxygen deficiency in MoO3 polycrystalline nanowires and nanotubes | |
WO2012101457A1 (en) | Exfoliation of layered materials | |
Taube et al. | Temperature induced phonon behaviour in germanium selenide thin films probed by Raman spectroscopy | |
Xing et al. | Solid–liquid–solid (SLS) growth of coaxial nanocables: silicon carbide sheathed with silicon oxide | |
Wang et al. | Nonlayered 2D ultrathin molybdenum nitride synthesized through the ammonolysis of 2D molybdenum dioxide | |
Wang et al. | Phase transition characteristics in the conductivity of VO 2 (A) nanowires: size and surface effects | |
Kargar et al. | Metallic vs. semiconducting properties of quasi-one-dimensional tantalum selenide van der Waals nanoribbons | |
Cole et al. | Structural, electronic, optical and vibrational properties of nanoscale carbons and nanowires: a colloquial review | |
Baek et al. | Creating nanostructured superconductors on demand by local current annealing | |
US11195634B2 (en) | Angstrom-scale nanowire arrays in zeolite | |
Zhong et al. | Mo6S3Br6: an anisotropic 2D Superatomic semiconductor | |
Chang et al. | Individual thermoelectric properties of electrodeposited bismuth telluride nanowires in polycarbonate membranes | |
Zhang et al. | Pressure-induced reversible structural phase transitions and metallization in GeTe under hydrostatic and non-hydrostatic environments up to 22.9 GPa | |
Hong et al. | Pressure-driven structural phase transitions and metallization in the two-dimensional ferromagnetic semiconductor CrBr 3 | |
Buh et al. | Template synthesis of single-phase δ3-MoN superconducting nanowires |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
FEPP | Fee payment procedure |
Free format text: ENTITY STATUS SET TO UNDISCOUNTED (ORIGINAL EVENT CODE: BIG.); ENTITY STATUS OF PATENT OWNER: SMALL ENTITY |
|
FEPP | Fee payment procedure |
Free format text: ENTITY STATUS SET TO SMALL (ORIGINAL EVENT CODE: SMAL); ENTITY STATUS OF PATENT OWNER: SMALL ENTITY |
|
AS | Assignment |
Owner name: KING ABDULLAH UNIVERSITY OF SCIENCE AND TECHNOLOGY, SAUDI ARABIA Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:LAI, ZHIPING;REEL/FRAME:048758/0223 Effective date: 20180703 Owner name: THE HONG KONG UNIVERSITY OF SCIENCE AND TECHNOLOGY, CHINA Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:SHENG, PING;ZHANG, BING;SIGNING DATES FROM 20180603 TO 20180703;REEL/FRAME:048758/0059 Owner name: KING ABDULLAH UNIVERSITY OF SCIENCE AND TECHNOLOGY Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:LAI, ZHIPING;REEL/FRAME:048758/0223 Effective date: 20180703 Owner name: THE HONG KONG UNIVERSITY OF SCIENCE AND TECHNOLOGY Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:SHENG, PING;ZHANG, BING;SIGNING DATES FROM 20180603 TO 20180703;REEL/FRAME:048758/0059 |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: DOCKETED NEW CASE - READY FOR EXAMINATION |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: NON FINAL ACTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: RESPONSE TO NON-FINAL OFFICE ACTION ENTERED AND FORWARDED TO EXAMINER |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: NON FINAL ACTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: RESPONSE TO NON-FINAL OFFICE ACTION ENTERED AND FORWARDED TO EXAMINER |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: NOTICE OF ALLOWANCE MAILED -- APPLICATION RECEIVED IN OFFICE OF PUBLICATIONS |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: PUBLICATIONS -- ISSUE FEE PAYMENT VERIFIED |
|
STCF | Information on status: patent grant |
Free format text: PATENTED CASE |